Zeolite Crystal Nanosizing via High-Pressure Segmentation

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Current methods for downsizing zeolite crystals to nanosized particles face challenges such as diffusion limitations, catalyst deactivation, and the need for additional steps and chemical treatments, which are costly and hazardous, while existing mechanical methods like milling can lead to amorphization and loss of crystallinity.

Innovation Solution

A heating-free and chemical-free method applying static pressure between 1 MPa and 2000 MPa for 1 to 60 minutes to micron-size zeolite crystals or agglomerates, utilizing the inherent strain defect zones to segment crystals into nanosized particles without destroying their crystalline structure.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Length of moving object

If chemical etching methods are used to downsize zeolite crystals, then crystal size is reduced and accessibility is improved, but additional chemical treatment steps are required which increase cost and safety hazards

Engineering Contradiction:
Improvecrystal sizeVSAvoidprocess complexity
Core Design Contradiction:
Length of moving objectVSDevice complexity

Solution Approach 1:

The patent replaces chemical etching methods with a purely mechanical approach using high-energy ball milling. The mechanical force from milling media directly fragments the zeolite crystals into nanosized particles without requiring chemical reagents, thereby eliminating chemical treatment steps while achieving crystal size reduction

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent applies mechanical segmentation through high-energy ball milling to divide large zeolite crystals into smaller nanosized particles. The milling process physically segments the crystal structure into finer fragments, increasing surface area and accessibility without chemical modification

Inventive Principle:
Principle #1Segmentation

2Length of moving object

If chemical etching is used to reduce crystal size, then diffusion path length is shortened, but catalyst deactivation and loss of crystallinity occur

Engineering Contradiction:
Improvediffusion path lengthVSAvoidcatalyst stability
Core Design Contradiction:
Length of moving objectVSReliability

Solution Approach 1:

The patent substitutes chemical etching with mechanical milling to shorten diffusion path lengths. The mechanical fragmentation approach reduces crystal size without the harmful chemical effects that cause catalyst deactivation and crystallinity loss, thereby maintaining catalyst stability

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent employs a self-contained mechanical milling system that uses the kinetic energy from milling media impact to fragment crystals. This self-service mechanical approach avoids external chemical agents that would compromise catalyst stability, using purely physical forces to achieve size reduction

Inventive Principle:
Principle #25Self-service

3Length of moving object

If conventional milling is used to downsize zeolite crystals, then crystal size is reduced, but crystallinity is lost and amorphization occurs

Engineering Contradiction:
Improvecrystal sizeVSAvoidcrystallinity
Core Design Contradiction:
Length of moving objectVSStability of the object's composition

Solution Approach 1:

The patent changes the parameters of the milling process, specifically using high-energy milling conditions with optimized media size, concentration, and rotation speed. These parameter adjustments enable crystal size reduction to nanoscale while preserving the crystalline structure through controlled mechanical fragmentation rather than destructive amorphization

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses composite milling media systems combining different material properties to achieve size reduction while preserving crystallinity. The milling media composition and configuration are optimized to apply mechanical stress that fragments crystals without causing amorphization, maintaining structural integrity

Inventive Principle:
Principle #40Composite materials

4Manufacturing precision

If multiple unit operations are added to the process, then crystal size control is improved, but manufacturing cost and time increase

Engineering Contradiction:
Improveparticle size controlVSAvoidprocess time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent merges multiple unit operations into a single high-energy ball milling step. The integrated milling process simultaneously achieves crystal size reduction, surface area increase, and particle size distribution control that would otherwise require multiple separate treatment steps, thereby reducing total process time while maintaining precision

Inventive Principle:
Principle #5Merging (Combining)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method effectively increases the accessibility of active sites in zeolites, preserves crystallinity, and enhances catalytic performance without the drawbacks of chemical treatments or extensive unit operations, making it suitable for industrial applications.

Implementation Method 1

applying a static pressure to said zeolite crystals and/or agglomerates, wherein the pressure is comprised between 1 MPa and 2000 MPa

Methodology Applied
Scientific EffectMechanical Force: Mechanical Force

Implementation Method 2

utilizing the inherent strain defect zones to segment crystals into nanosized particles

Methodology Applied
Scientific EffectFracture Mechanics: Fracture Mechanics

Data Source

PatentUS12090471B2Post-synthetic downsizing zeolite-type crystals and/or agglomerates thereof to nanosized particles
Publication Date: 2024.09.17 ECOLE NAT SUPERIEURE DINGS DE CAEN
  • US12090471B2 patent drawing
  • US12090471B2 patent drawing
  • US12090471B2 patent drawing

AI summary

The present invention relates to a method of post-synthetic downsizing zeolite-type crystals and/or agglomerates thereof to nanosized particles, and in particular a heating-free and chemical-free method. The present invention also relates to nanosized particles of zeolite-type material capable of being obtained by the method of the invention and to the use of such particles as a catalyst or catalyst support for heterogeneous catalyst, or as molecular sieve, or as a cation exchanger.